JPH10106352A - Paste and its manufacture - Google Patents
Paste and its manufactureInfo
- Publication number
- JPH10106352A JPH10106352A JP28015796A JP28015796A JPH10106352A JP H10106352 A JPH10106352 A JP H10106352A JP 28015796 A JP28015796 A JP 28015796A JP 28015796 A JP28015796 A JP 28015796A JP H10106352 A JPH10106352 A JP H10106352A
- Authority
- JP
- Japan
- Prior art keywords
- particles
- paste
- raw material
- water
- organic solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
Landscapes
- Colloid Chemistry (AREA)
- Conductive Materials (AREA)
Abstract
Description
【0001】[0001]
【発明の属する技術分野】この発明は、品質を向上させ
ながら製造コストを低減可能にするペースト及びその製
造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a paste and a method for producing the same, which can reduce the production cost while improving the quality.
【0002】[0002]
【従来の技術】ペーストには大別して、導体ペースト、
抵抗ペースト、及び誘電体ペーストの三種類が有る。導
体ペーストは、電気回路や電極用の焼成膜を形成するも
ので、金ペースト、銀ペースト、銀合金ペースト、銅ペ
ースト、銅合金ペースト等が用いられる。抵抗ペースト
は、電気回路形成用の抵抗素子やヒータ等を焼成形成す
るために用いられるもので、白金系ペースト、白金合金
系ペースト、ルテニウム系ペースト等が有る。又、誘電
体ペーストは、電気回路や電極表面の絶縁、コンデンサ
素子の電極間誘電体、ヒータ表面の絶縁、或いは回路素
子、センサ類、定着ローラ他の機器の被覆用として用い
られ、主にガラス類が原材料として用いられる。2. Description of the Related Art Pastes are roughly divided into conductive pastes,
There are three types, a resistance paste and a dielectric paste. The conductive paste forms a fired film for an electric circuit or an electrode, and may be a gold paste, a silver paste, a silver alloy paste, a copper paste, a copper alloy paste, or the like. The resistance paste is used for firing and forming a resistance element, a heater, and the like for forming an electric circuit, and includes a platinum-based paste, a platinum alloy-based paste, a ruthenium-based paste, and the like. In addition, dielectric paste is used for insulation of electric circuits and electrode surfaces, dielectric between electrodes of capacitor elements, insulation of heater surfaces, or coating of circuit elements, sensors, fixing rollers and other devices, and is mainly used for glass. Are used as raw materials.
【0003】金ペースト、銀ペースト他の導体ペースト
は、主原料として金属粒子が用いられている。例えば、
金粒子を得るためには、金塊を王水中に投入して溶解さ
せた後、ここに還元水を加えて還元させて金粒子を析出
させた後、これを洗浄してから乾燥して水分を飛ばして
金粒子を得る。銀粒子も類似の化学的方法により得る事
が出来る。かくして得られた金属粒子は、ガラスフリッ
ト、樹脂、その他の添加物と共に有機溶媒中に分散させ
て導体ペーストを得る。この分散のためにロールやブレ
ンダーが用いられる為、乾燥金属粒子が二次凝集したま
ま押圧されて部分的に箔状になり、製品不良を生ずるこ
とが有った。また、抵抗ペーストにおいても、乾燥金属
粒子の凝集によって製品不良を生ずる可能性が有った。[0003] Gold paste, silver paste and other conductive pastes use metal particles as a main raw material. For example,
In order to obtain the gold particles, the gold lumps are put into aqua regia and dissolved, and then reduced water is added thereto to reduce the gold particles.Then, the gold particles are precipitated, washed and dried to remove the water. Skip to get gold particles. Silver particles can also be obtained by similar chemical methods. The metal particles thus obtained are dispersed in an organic solvent together with a glass frit, a resin, and other additives to obtain a conductive paste. Since a roll or a blender is used for this dispersion, the dried metal particles are pressed while being secondary-agglomerated and partially formed into a foil, which may cause a defective product. Also, in the case of the resistance paste, there was a possibility that a defective product would be caused by agglomeration of the dried metal particles.
【0004】誘電体ペーストの場合は、ガラスやセラミ
ックス等を10μm程度の粒径まで粉砕するためにボー
ルミル工程が必要となる。このボールミルポットからの
原料のディスチャージの際に水性液が用いられる上、原
料が水に濡れてしまい、これまた乾燥工程が必要とな
る。この乾燥でガラス類等は再び塊状になってしまい扱
いにくいものとなる。[0004] In the case of a dielectric paste, a ball mill process is required to grind glass, ceramics, and the like to a particle size of about 10 µm. In discharging the raw material from the ball mill pot, an aqueous liquid is used, and the raw material becomes wet with water, which also requires a drying step. By this drying, the glass and the like again become lump and difficult to handle.
【0005】[0005]
【発明が解決しようとする課題】この様に、従来技術に
よれば、必ず原料粒子の乾燥工程がついてまわり、多大
な乾燥空間を要するばかりか、多大な費用と時間とを要
するものであった。そればかりか、ペースト中の原料粒
子の分散性も充分でなく、金属粒子にあっては乾燥によ
って二次凝集することもあった。特に、金粒子の様に軟
質粒子においては、その可能性が高かった。As described above, according to the prior art, the process of drying the raw material particles is always involved, and not only a large amount of drying space is required but also a large amount of cost and time are required. In addition, the dispersibility of the raw material particles in the paste was not sufficient, and the metal particles were sometimes secondary-aggregated by drying. In particular, the possibility was high for soft particles such as gold particles.
【0006】そこでこの発明は、ペースト中の原料粒子
の分散性を良くして焼成膜の品質の向上を図ると共に、
製造コストの低減を図ることを目的とする。Therefore, the present invention aims to improve the quality of the fired film by improving the dispersibility of the raw material particles in the paste,
The purpose is to reduce the manufacturing cost.
【0007】[0007]
【課題を解決するための手段】この発明の目的は、少な
くとも主原料粒子の表面を親油化して有機溶媒中に分散
させてなるペーストによって達成される。この発明の目
的は、主原料粒子は金属粒子或いはガラス粉末粒子であ
ることを特徴とする「請求項1」のペーストによって達
成される。又、この発明の目的は、金属粒子水性ディス
パージョンに界面活性剤を投入して金属粒子の表面を親
油化した後、水より比重の大きな油水分離溶剤を投入し
て水を除去し、しかる後に容易に揮発しない有機溶媒を
投入してから前記油水分離溶剤を揮発させて置換し、前
記親油化した金属粒子を有機溶媒中に分散させるペース
トの製造方法によって達成される。この発明の目的は、
金属粒子は金粒子であることを特徴とする「請求項4」
のペーストの製造方法によって良好に達成される。この
発明の目的は、少なくとも一種類の水にぬれた原料粒子
の表面を親油化処理してから水よりも比重の大きな油水
分離溶剤と混合して水を除去し、しかる後に容易に揮発
しない有機溶媒を投入してから前記油水分離溶剤を揮発
させて置換し、前記親油化した原料粒子を有機溶媒中に
分散させるペーストの製造方法によって達成される。更
に、この発明の目的は、少なくとも一種類の原料粒子の
表面を親油化処理してから有機溶媒中に分散させるペー
ストの製造方法によって達成される。The object of the present invention is attained by a paste obtained by lipophilizing at least the surface of the main raw material particles and dispersing the particles in an organic solvent. The object of the present invention is attained by a paste according to claim 1 wherein the main raw material particles are metal particles or glass powder particles. Further, an object of the present invention is to add a surfactant to an aqueous dispersion of metal particles to make the surface of the metal particles lipophilic, and then add an oil / water separation solvent having a higher specific gravity than water to remove water. This is achieved by a method for producing a paste in which an organic solvent that is not easily volatilized later is charged and then the oil-water separation solvent is volatilized and replaced, and the lipophilic metal particles are dispersed in the organic solvent. The purpose of this invention is
(Claim 4) wherein the metal particles are gold particles.
Satisfactorily achieved by the method for producing a paste of the present invention. An object of the present invention is to lipophilicize the surface of at least one kind of water-wetted raw material particles and then remove the water by mixing with an oil-water separation solvent having a higher specific gravity than water, and thereafter not easily volatilized. This is achieved by a method for producing a paste in which an oil-water separation solvent is volatilized and replaced after an organic solvent is charged, and the lipophilic raw material particles are dispersed in the organic solvent. Further, the object of the present invention is achieved by a method for producing a paste in which the surface of at least one kind of raw material particles is subjected to lipophilic treatment and then dispersed in an organic solvent.
【0008】[0008]
【発明の実施の形態】この発明によれば、少なくとも一
種類の原料粒子の表面を親油化処理後、水よりも比重の
大きな油水分離溶剤を投入して水を除去し、しかる後に
容易に揮発しない有機溶媒を投入してから前記油水分離
溶剤を揮発させて置換し、親油化した原料粒子を有機溶
媒中に分散させてペーストを得るものであるので、原料
粒子が良好に分散して二次凝集を生ずることが無くなる
ばかりか、原料粒子の乾燥工程が不要となり、製造工程
が簡略化出来るものとなる。主原料粒子が金のごとく柔
らかい材質である場合には、不良率が極めて小さくなる
ので、特に有効である。原料粒子としては、各種の金属
粒子やガラス粉末粒子を用いる事が出来る他、市販の乾
燥した原料粒子も、その表面を親油化することにより、
この発明を適用する事が出来る。According to the present invention, after the surface of at least one kind of raw material particles is subjected to lipophilic treatment, an oil / water separation solvent having a higher specific gravity than water is introduced to remove water, and thereafter, easily. Since the oil-water separation solvent is volatilized and replaced by introducing a non-volatile organic solvent, the paste is obtained by dispersing the lipophilic raw material particles in the organic solvent, so that the raw material particles are well dispersed. Not only does the secondary agglomeration not occur, but also the step of drying the raw material particles becomes unnecessary, and the manufacturing process can be simplified. It is particularly effective when the main raw material particles are made of a soft material such as gold, because the defective rate becomes extremely small. As the raw material particles, various metal particles and glass powder particles can be used, and also commercially available dried raw material particles, by making the surface lipophilic,
The present invention can be applied.
【0009】ガラス粉末粒子類、セラミック粉末粒子類
を得るために、ボールミル内に原料を投入して粉砕する
が、これを取り出す際に水等を用いるので、粒子が濡れ
てしまうため、これを乾燥し、この際固化したものを再
び粉末状にするのは非常にわずらわしく、時間と費用を
要する。そこでこの発明においては、濡れた原料粒子を
乾燥することなく、粒子表面を直接親油化してから油水
分離溶剤と混合して分離した水を除き、この油水分離溶
剤と有機溶媒とを置換して、粒子を溶媒中に分散させて
ペーストを得る。そのため、乾燥の段取りが不要とな
り、流れの良い製造を行える。又、この発明によれば、
粒子表面が親油化されるので、粒子が溶媒中で二次凝集
することが無く、粒径0.5μm以下の原料であっても
問題なく用いることが可能であり、その分焼成膜品質の
向上と用途拡大の自由度の大きなペーストを製造できる
ものとなる。In order to obtain glass powder particles and ceramic powder particles, the raw materials are put into a ball mill and pulverized. However, since water and the like are used when taking out the particles, the particles are wetted. At this time, it is very troublesome to re-solidify the solidified powder, which requires time and cost. Therefore, in this invention, without drying the wet raw material particles, the surface of the particles is directly lipophilic and then mixed with an oil-water separation solvent to remove the water separated, and the oil-water separation solvent and the organic solvent are replaced. The particles are dispersed in a solvent to obtain a paste. Therefore, the preparation for drying becomes unnecessary, and the production with good flow can be performed. According to the invention,
Since the particle surface is made lipophilic, the particles do not undergo secondary aggregation in the solvent, and even a raw material having a particle size of 0.5 μm or less can be used without any problem. It is possible to produce a paste having a high degree of freedom for improvement and application expansion.
【0010】更に、この発明による製造方法において一
部の添加物としてあらかじめ乾燥した材料粒子を用いる
場合、或いは乾燥粒子のみでペーストを製造する場合に
は、乾燥粒子の表面を親油化してから有機溶媒に分散さ
せることができる。[0010] Further, in the production method according to the present invention, when previously dried material particles are used as a part of the additive, or when a paste is produced using only the dried particles, the surface of the dried particles is made lipophilic and then the organic material is removed. It can be dispersed in a solvent.
【0011】[0011]
【実施例】先ず、99.99%以上の純度を持った金1
Kgを4リットルの王水に投入して溶解させた後、これ
に還元剤として40リットルの塩化ヒドロキシルアミン
を投入して金粒子を還元析出させて45リットルの金粒
子水性ディスパージョンを得た。この金粒子水性ディス
パージョン中に界面活性剤としてドデシルアミン80g
を加えて溶解させて、析出金粒子の表面を親油化させ
た。尚、界面活性剤の投入タイミングは、金粒子水性デ
ィスパージョン完成後に限定されるものでは無く、還元
剤投入前、或いは還元剤投入と同時に投入して、金粒子
の還元析出と同時に金粒子の表面を親油化するようにし
ても良い。EXAMPLE First, gold 1 having a purity of 99.99% or more was used.
After Kg was poured into 4 liters of aqua regia to dissolve it, 40 liters of hydroxylamine chloride as a reducing agent was added thereto to cause gold particles to be reduced and precipitated to obtain 45 liters of an aqueous dispersion of gold particles. 80 g of dodecylamine as a surfactant in the aqueous dispersion of gold particles
Was added and dissolved to make the surface of the precipitated gold particles lipophilic. The timing of the addition of the surfactant is not limited after completion of the aqueous dispersion of gold particles, and is added before or simultaneously with the addition of the reducing agent, and the surface of the gold particles is added simultaneously with the reduction and precipitation of the gold particles. May be made lipophilic.
【0012】界面活性剤を加えた金粒子水性ディスパー
ジョンを一昼夜放置し、表面が親油化された金粒子を自
然沈下させて上澄み液を抜き取り、約4リットルまで濃
縮した。この濃縮された金粒子水性ディスパージョン4
リットル中に、水よりも比重の大きな油水分離溶剤とし
てのパークロロエチレン3リットルを投入した。この状
態では、金粒子表面に親水基が吸着すると共に親油基が
外側に向く界面活性剤は、その親油基によってパークロ
ロエチレンに良く濡れ、水はパークロロエチレンの上に
浮く。そこで、ゆっくりと攪拌して水を全部追い出して
上部に浮かせて除去し、金粒子表面を完全に親油化す
る。次いで、パークロロエチレン中に金粒子の分散した
金粒子油性デイスパージョンを放置して金粒子を沈下さ
せて上澄み液を抜き取り、数十cc程度まで濃縮した。
この濃縮油性ディスバージョンに、容易に揮発しない有
機溶媒としてターピネオイル3リットルを加え、攪拌し
た後静置して上澄み液を抜き取り、これを3回繰り返し
た。その後、更に澄みでてくる有機溶媒を可能な限り吸
い取り、金粒子の含有率を90%以上とした。この間
に、パークロロエチレンからなる油水分離溶剤は揮発し
た。尚、油水分離溶剤としては、パークロロエチレンの
他に、クロロホルム、メチレンクロライド、フレオン類
等があり、金属粒子の粒径他の条件によって使いわけら
れる。The aqueous dispersion of gold particles to which a surfactant was added was allowed to stand overnight, and the gold particles having a lipophilic surface were spontaneously settled, the supernatant was removed, and concentrated to about 4 liters. This concentrated aqueous dispersion of gold particles 4
In the liter, 3 liters of perchlorethylene as an oil-water separation solvent having a specific gravity larger than that of water was charged. In this state, the surfactant whose hydrophilic group is adsorbed on the surface of the gold particles and whose lipophilic group faces outward is well wetted by perchlorethylene by the lipophilic group, and water floats on the perchlorethylene. Therefore, the water is completely stirred to drive out all the water and floated at the top to remove it, thereby completely lipophilicizing the surface of the gold particles. Next, the gold particle oily dispersion in which the gold particles were dispersed in perchlorethylene was left to settle the gold particles, a supernatant liquid was drawn out, and concentrated to about several tens cc.
To this concentrated oily dispersion was added 3 liters of terpine oil as an organic solvent which was not easily volatilized. After stirring, the mixture was allowed to stand, and the supernatant was taken out. This was repeated three times. Thereafter, as much of the clear organic solvent as possible was sucked out, and the content of gold particles was set to 90% or more. During this time, the oil-water separation solvent composed of perchlorethylene volatilized. In addition, as the oil-water separation solvent, there are chloroform, methylene chloride, freons, and the like in addition to perchlorethylene, and they are used depending on other conditions such as the particle size of the metal particles.
【0013】その後、90%の金粒子を内在する有機溶
媒中に、必要に応じてガラスフリット、無機添加物、樹
脂類等を適量加えて、金粒子の重量パーセントを80%
から85%としてから、ロールやブレンダー等の機械に
かけて金粒子を有機溶媒中に分散させる。この際、金粒
子の表面は親油化されているので二次凝集を生ずること
は無く、良好に分散されたペーストを得る事ができる。
ここで得られた金ペーストをスクリーンを用いて基板上
に印刷してから焼成して評価した所、導体抵抗値は3.
5mΩ/□(膜厚10μm)、表面粗さは0.316μ
m、密着力は3.8Kg/4mm2であり、同一の金粒
子径、同一の添加物の従来方式の金ペースト(乾燥金粒
子使用)の導体抵抗値5.1mΩ/□(膜厚10μ
m)、表面粗さ0.457μm、及び密着強度2.6K
g/4mm2であった点と比較すると、導体抵抗値は3
1.4パーセント低下し、表面粗さは30.9パーセン
ト低下し、密着力は46.2パーセント向上したことに
なる。Thereafter, an appropriate amount of a glass frit, an inorganic additive, a resin or the like is added to an organic solvent containing 90% of the gold particles, if necessary, to reduce the weight percentage of the gold particles to 80%.
After that, the gold particles are dispersed in an organic solvent using a machine such as a roll or a blender. At this time, since the surface of the gold particles is made lipophilic, secondary aggregation does not occur and a well-dispersed paste can be obtained.
When the obtained gold paste was printed on a substrate using a screen and then fired, the conductor resistance was 3.
5mΩ / □ (film thickness 10μm), surface roughness 0.316μ
m, the adhesion is 3.8 kg / 4 mm 2 , and the conductor resistance value of the conventional gold paste (using dry gold particles) of the same gold particle diameter and the same additive is 5.1 mΩ / □ (film thickness of 10 μm).
m), surface roughness 0.457 μm, and adhesion strength 2.6 K
g / 4 mm 2 , the conductor resistance value is 3
A 1.4% reduction, a 30.9% reduction in surface roughness and a 46.2% improvement in adhesion.
【0014】ペーストに用いる主原料粒子としては、上
記の実施例に示した様な金粒子等の金属粒子の他、ガラ
ス粉末粒子やセラミック粉末粒子等を用いることができ
る。又、金属粒子としては、合金粒子でも良いが、例え
ば銀−パラジウムペーストのごとく、銀とパラジウムと
を別々に溶解還元析出させた各粒子を、別々に親油化
し、これらを適量ずつ混合して油水分離、或いは油水分
離してから混合する等の方法を用いても良い。白金−パ
ラジウムペースト、白金−ロジウムペースト等は、合金
を用いた方が効率的である。As the main raw material particles used for the paste, glass powder particles, ceramic powder particles, and the like can be used in addition to metal particles such as gold particles as shown in the above-described embodiment. Further, as the metal particles, alloy particles may be used.For example, like silver-palladium paste, particles obtained by separately dissolving and reducing silver and palladium are separately made lipophilic, and these are mixed in appropriate amounts. A method such as oil-water separation or oil-water separation followed by mixing may be used. It is more efficient to use an alloy such as a platinum-palladium paste or a platinum-rhodium paste.
【0015】[0015]
【発明の効果】以上の通りこの発明によれば、乾燥工程
が省略出来るので、製造コストが低減されるばかりか、
均一分散しているので粘度の急変等の異常が生ずる事が
なく、製造しやすくなる。また、この発明の方法によっ
て得られたペーストは、粒子が均一分散しているため基
板への焼成膜の密着力が大きくなると共に表面粗さも低
減され、導体ペーストにあっては導体抵抗が低減され、
抵抗ペーストにあっては抵抗値の不均一問題やそれによ
る局部的静電破損も生じなくなり、また誘電体ペースト
にあっては安定した絶縁特性が得られる等品質が一段と
向上する効果が得られる。As described above, according to the present invention, since the drying step can be omitted, not only the manufacturing cost is reduced, but also
Since it is uniformly dispersed, there is no occurrence of abnormalities such as a sudden change in viscosity, and the production becomes easy. Further, in the paste obtained by the method of the present invention, since the particles are uniformly dispersed, the adhesion of the fired film to the substrate is increased and the surface roughness is reduced, and in the case of the conductor paste, the conductor resistance is reduced. ,
In the case of the resistance paste, the problem of non-uniformity of the resistance value and the local electrostatic damage due to the problem are not caused, and in the case of the dielectric paste, the effect that the quality is further improved such as stable insulation characteristics can be obtained.
Claims (7)
て有機溶媒中に分散させてなるペースト。1. A paste obtained by lipophilizing at least the surface of main raw material particles and dispersing the particles in an organic solvent.
とする「請求項1」のペースト。2. The paste according to claim 1, wherein the main raw material particles are metal particles.
を特徴とする「請求項1」のペースト。3. The paste according to claim 1, wherein the main raw material particles are glass powder particles.
性剤を投入して金属粒子の表面を親油化した後、水より
比重の大きな油水分離溶剤を投入して水を除去し、しか
る後に容易に揮発しない有機溶媒を投入してから前記油
水分離溶剤を揮発させて置換し、前記親油化した金属粒
子を有機溶媒中に分散させるペーストの製造方法。4. An aqueous dispersion of metal particles is charged with a surfactant to lipophilize the surface of the metal particles, and then an oil-water separation solvent having a specific gravity greater than that of water is charged to remove water. A method for producing a paste in which an organic solvent that does not volatilize is charged, the oil-water separation solvent is volatilized and replaced, and the lipophilic metal particles are dispersed in an organic solvent.
する「請求項4」のペーストの製造方法。5. The method according to claim 4, wherein the metal particles are gold particles.
の表面を親油化処理してから水よりも比重の大きな油水
分離溶剤と混合して水を除去し、しかる後に容易に揮発
しない有機溶媒を投入してから前記油水分離溶剤を揮発
させて置換し、前記親油化した原料粒子を有機溶媒中に
分散させるペーストの製造方法。6. The method of claim 1, wherein the surface of the raw material particles wetted with at least one kind of water is lipophilized and then mixed with an oil / water separation solvent having a higher specific gravity than water to remove water. A method for producing a paste, in which a solvent is added, the oil-water separation solvent is volatilized and replaced, and the lipophilic raw material particles are dispersed in an organic solvent.
油化処理してから有機溶媒中に分散させるペーストの製
造方法。7. A method for producing a paste wherein at least one kind of raw material particles is subjected to lipophilic treatment and then dispersed in an organic solvent.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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JP28015796A JP3739147B2 (en) | 1996-09-30 | 1996-09-30 | Paste and manufacturing method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP28015796A JP3739147B2 (en) | 1996-09-30 | 1996-09-30 | Paste and manufacturing method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH10106352A true JPH10106352A (en) | 1998-04-24 |
JP3739147B2 JP3739147B2 (en) | 2006-01-25 |
Family
ID=17621117
Family Applications (1)
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---|---|---|---|
JP28015796A Expired - Lifetime JP3739147B2 (en) | 1996-09-30 | 1996-09-30 | Paste and manufacturing method thereof |
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Country | Link |
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JP (1) | JP3739147B2 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2001057885A1 (en) * | 2000-01-31 | 2001-08-09 | Toho Titanium Co., Ltd. | Nickel power dispersion, method of producing nickel power dispersion and method of producing conductive paste |
CN100454444C (en) * | 2001-08-21 | 2009-01-21 | Tdk株式会社 | Conductive paste composition, conductive paste and its preparation |
-
1996
- 1996-09-30 JP JP28015796A patent/JP3739147B2/en not_active Expired - Lifetime
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2001057885A1 (en) * | 2000-01-31 | 2001-08-09 | Toho Titanium Co., Ltd. | Nickel power dispersion, method of producing nickel power dispersion and method of producing conductive paste |
EP1195773A1 (en) * | 2000-01-31 | 2002-04-10 | Toho Titanium Co., Ltd. | Nickel power dispersion, method of producing nickel power dispersion and method of producing conductive paste |
US6620220B2 (en) | 2000-01-31 | 2003-09-16 | Toho Titanium Co., Ltd. | Nickel powder dispersion, method of producing nickel power dispersion and method of producing conductive paste |
EP1195773A4 (en) * | 2000-01-31 | 2009-01-28 | Toho Titanium Co Ltd | Nickel power dispersion, method of producing nickel power dispersion and method of producing conductive paste |
CN100454444C (en) * | 2001-08-21 | 2009-01-21 | Tdk株式会社 | Conductive paste composition, conductive paste and its preparation |
Also Published As
Publication number | Publication date |
---|---|
JP3739147B2 (en) | 2006-01-25 |
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